Apparatus for carrying out reactions continuously in the liquid phase under increased pressure



p 13, 1932- K. H. SAUNDERS APPARATUS FOR CARRYING OUT REACTIONS CONTINUOUSLY IN THE LIQUID PHASE UNIIIJER INCREASED PRESSURE Filed Oct. 29. 1928 /NVENTOR.,

K5 lV/VETH Hum 51? dbl/M05126,

IBY

Patented Sept. 13, 1932 Q UNDEB. monnnsnn PRESSURE Application filed October 29,

3 In the art of continuous chemical processes it is well known to bring about a reaction in a liquid solution or suspensionby forcing, the same through a coiled pipe heated by a suitable source. If the process is carried out above the boiling point of one or more of the constituent liquids pressure will be set up and special means must be adopted for regulating the same. hitherto been done in either of t viz: (1) by attaching to the system an hydraulic accumulator by which device a' steady working pressure is. maintained, or (2) .by adjusting the inlet and outlet valves so that the inflow of materials is exactly balanced against outflow. Both devices are unsatisfactory in practice, the former because an accumulator is an expensive apparatus liable to fail in chemical work by corrosion, to permit leakage of dangerous material or become blockedfby crystalliza- The latter device requires continuous personal attention to maintain pressure balance particularly in systems of small capacityand there always remains present the possibilitiesof either acomplete discharge of the reaction liquids or the. generation of a dangerously high pressure. I v I have designed, perfected and made a new device or apparatus which .is suitable for continuously effecting such chemical reactions in the liquid phase at high temperatures and vated pressure. I My new apparatus com prises a closed container or surrounding, vessel capable of withstanding high internal wo ways,

pressures, this container being. divided in-;

ternally into two separate reaction chambers and having a substantial vapor space above said reaction chambers and in direct communication with them. This vapor space is the means by which the pressure within said closed container may be easily, effectively and advantageously maintained substantiallv uniform and controlled. Thevapor space balances ordinary fluctuations incidentalto the normal process. To assist in controlling the pressure, both in in providing against extraordinary fluctuations in pressure, I provide means for with- 'arate internal reaction chambers and. delicate I under substantially uniform .ele-- atube 8. The elements 5 and starting the process and CONTINUOUSLY 192s. Seria1,1\To.315,906.

drawing vapors from said'vapor space to control the pressure at such times. [The separe so arranged that theyare in free unrestrictedtcommunication with each other. By this arrangement the liquid reaction mixture may freely overflow from one chamberinto the other. My new apparatus is provided with suitable means for introducing and withiinner reaction chamber as maybe desired.

it is advantageous to overflow of the liquid reaction mixture. In the accompanying illustration I, have shown,-more. or less diagrammatically,- an embodiment, of my invention useful in the performance of the described process. In this showing the figure is a view in vertical: section with certain parts in elevation. I

'Referring'to the structure shownin Fig-,- ure 1, element 1 is a reaction vessel'suitable. for retaining high pressures. It is closed at; both ends by lens ring joints 2. A vertically. disposed central tube, open at the top, is shown at 3 leaving an v tween the walls of the reaction vesseL- The lower section of the annular space4 may be filled with Raschig rings 12surmounted by a distributor plate 13, into which may dip 10 are tubes leading to the lens. ring joints, while ele-v tive inlet and outletpipes. f

In-use, the reaction vessel may be heated or cooled by suitable means.

ments 6, 7, 9 and llare valves in the respecried out, can be forced in through the pipe annular space 4 .be-

5, at the bottom of the annular space and will rise up therein until eventually it overflows into the vessel 8 from the bottom of which it is drawn off by the outlet valve 6. The length of the pressure vessel and the speed of flow are adjusted sothat the reaction is complete when theliquid overflows. It will be seen that this simple apparatus overcomes the difficulties mentioned above, for the tube 3 and vapour space above it fulfill the duties of an hydraulic accumulator by. allowing the pressure to remain constant while the liquid volume varies. A device adapted to give a warning when the central tube has become full is advantageously, employed.

A second liquid may be injected by way of the valve 7 and pipe 8 leading into the annular space 4. If this liquid and its reaction products are heavier than the first liquid and immiscible therein, a counter-current action results and the new product can be drawn off by the valve 9, while the spent liquor flows away by the outlet 6. Alternatively, ifit is desired to protect the pressurecontaining walls against an exothermic reaction, the central tube 3 may be made larger than shown, the reacting materials may be injected-in it by way of the valve 6 and the product may be allowed to overflow into the annu-' lar space 4 to be drawn off therefrom by the valve 9. A pipe 10 leads to a pressure gauge; anotherpipe 11 may be used as outlet for gaseous reaction products. The actual arrangement and relative dimensions of the apparatus may be varied within wide limits and the above description is to be considered illustrative and not limitative.

E mample :The annular 7 two-thirds of the way up with Raschig rings surmounted by a distributor plate consisting of an annular perforated ring, into which the inlet tube 8 dips. Aqueous ammonia, preferably having a specific gravity of 0.880, is forced in continuously and heated until the pressure reaches to 100 atmospheres. 'Molten p-chloronitrobenzene is forced into the ammonia stream by means of the pipe 8 at such a rate that none reaches the bottom of the annular space, but all is converted into p-nitroaniline which overflows into the central tube with the ammonia and is drawn off at 6 in solution in theammonia stream, and isolated in any convenient-manner.

' WVhat Iclaim and ters Patent is 1. An apparatus for carrying out reacdesire to secure by Lettions continuously. in the liquid phase under,

increased pressure, comprising two concentric chambers, the inner one being without a top, so that there is a space at the top common to both chambers, inlet and outlet pipes for the admission of the reagents and the exit of the reaction products, means for heatspace is filled.

through the pipe 5 ing or cooling the outer chamber, an inlet pipe and an outlet pipe opening at the bottom of the outer chamber, a pipe opening at the bottom of the inner chamber, a p pe passing through the cover and descending into the outer chamber, below the open topof the inner'chamber, and an additional outlet pipe opening at the common space at the top of the twochambers, the annular space being partly filled: with Raschig rings s11r mounted by a distributor plate into which dips the pipe passing through the'cover and descendinginto the outer chamber, said distributor plate consisting of an annular perforatedring.

2. An apparatus for continuously effecting reactions in'the liquid-phase under increased pressure, said apparatus comprising, two reaction chambers, oneof said chambers ens closing the other, the inner'chamber in open unrestrictedcommunication with the outer chamber, a substantial vaporspace common to both chambers, thus permitting liquid reaction mixtures to freely flow from one chamber to the other without sealing said vapor space from said'chambers, means for introducing and withdrawing liquid reaction mixtures into and out of said chainbers, and means for controlling the pressure in said vapor'space.

3. An apparatus for continuouslyeffecting reactions in the liquid phase under increased pressure, the-said: apparatus comprising two separate reaction chambers, one disposed within the other, the outer" chamber having walls capable of withstanding relatively high pressures, saidinner chamber being so disposed in the outer chamber as to leave a relatively large vapor space common to both chambers andpermit reaction mixture from one chamber to the other without sealing. said vapor space, means for introducing and withdrawing reaction mixtures into and out of. said chambers, said vapor space, andmeans for regulating the temperatures within said chambers.

i. An apparatus for continuously effecting reactions in the liquid phase under increased pressure, said-apparatus comprising a closed pressure resistingcontainer divided into two reaction chambers, said reaction chambers being in open unrestricted communication with each other and having a relatively large vapor space for'introducing a liquid reaction mixture into one of'the said reactionchambers, said means being such that the liquid reaction mixture is forcedthrough the first" reaction chamber'and overflowsinto the" second reaction chamber, means for removing said liquid'reaction mixture fromthe saidsec- 0nd reaction chamber,

and means for removingvapors from the being free flow of a liquid.

means for controllingthe pressure 1n common to both, means means for controlling the temperature in said reaction chambers.

reactlons in the liquid phase at high tem perature and under substantially uniform elevated pressures, said apparatus comprising a closed pressure resisting cylindrical container, said container being divided by an internal cylindrical wall into two con-' centric reaction chambers, said reaction chamber being closed at the bottom and open at the top, the said opening at the top being so arranged to provide a substantial vapor space common to both reaction chambers and mixture from one reaction chamber to the ther, means for introducing a liquid reactant under pressure into the outer reaction chamber, means for introducing a second reactant against pressure into said outer chamber, means for withdrawing the liquid re action product from the inner reaction chamber, from said vapor space to control the sure in said closed container, and means for controlling the temperature within said closed container. 7

6. An apparatus for continuously effecting chemical reactions in the liquid phase at high tem aeratures and substantially uniform elevated pressures, said apparatus comprising a closed cylindrical container capable of withstanding relatively high internal pressures, a cylindrical wall centrally disposed in said container thereby forming an outer and an inner reaction chamber, a vapor space above said reaction chambers, space being common to both reaction chambers and in direct communication with each of said reaction chambers, means for introducing a liquid reaction mixture in the bottom of said inner reaction chamber, said means being such that the said liquid reaction mixture is forced upward in the chamber causing the reaction mixture to freely overflow into said outer chamber, means for withdrawing said liquid reaction mixture from the bottom of said outer chamber, and means for withdrawing vapors from said vapor space to control the pressure within said closed container.

7 n apparatus for continuously effecting chemical reactions in the liquid phase under substantially v uniform increased pressure, said apparatus comprising a vertical tubular member, with closing members positioned at each end of said tubular member and securely secured thereto, sealing members positioned between said closing memsaid Vertical 'bular member permit free overflow of a liquidreaction means for withdrawing vaporspres-v f tinuously overflow tubular memher for sealingthe joints between such members, said assembled members forming a closed pressure resisting container, a second vertically disposed tubular member mounted and secured to the lower closing member, the second tubular member being closed at the bottom by the lower closing,

member and open at the top, the second tubeing shorter than the first tubular member, thus container into two reaction chambers one tion chambers, an aperture in the upper closvertical tubular member, apertures in the the pressure in said-Va apparatus being readily isassembled and re assembled for inspection and cleaning.

8. The process of continuously effecting reactions in liquid phase in which the liquid products formed are soluble in the reaction mixture, which tively narrow vertical column of a liquid reaction mixture, maintaining said column at reaction temperature, thereby effecting the reaction within said or space, the said llqllld reaction mixture,

umrli lnto an outlet zone laterally of the vertica liquid reaction products;

In testimony whereof I aflix my signature. KENNETH HERBERT SAUNDERS.

dividing the said closed,

comprises forming a rela- 

